反应详情

A solution of Example 270 (1.4192 g, 3.77 mmol) in methanol (20 mL) was added to Raney-nickel (14.1 g). The vessel was pressurized to 60 psi with H2 and shaken for 5 hours. The reaction was then filtered and concentrated to yield the desired product (1.18 g, 90%). MS (ESI(+)) m/e 332 (M+H)+, 364 (M+NH4)+, 369 (M+Na)+; MS (ESI(−)) m/e 345 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 7.48 (d, 1H), 7.17 (t, 1H), 6.92 (d, 1H), 6.80 (d, 1H), 6.71 (d, 3H), 6.52 (t, 1H), 2.92 (m, 2H), 2.58 (m, 2H), 1.60 (m, 4H).

1. filtrationThe reaction was then filtered
2. concentrationconcentrated